CN110462113A - The manufacturing method of III nitride semiconductor substrate and III nitride semiconductor substrate - Google Patents

The manufacturing method of III nitride semiconductor substrate and III nitride semiconductor substrate Download PDF

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Publication number
CN110462113A
CN110462113A CN201880021145.6A CN201880021145A CN110462113A CN 110462113 A CN110462113 A CN 110462113A CN 201880021145 A CN201880021145 A CN 201880021145A CN 110462113 A CN110462113 A CN 110462113A
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China
Prior art keywords
nitride semiconductor
iii nitride
main surface
growth
axis
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后藤裕辉
石原裕次郎
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Furukawa Desk Metal Co Ltd
Furukawa Co Ltd
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Furukawa Desk Metal Co Ltd
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Abstract

The present invention provides a kind of III nitride semiconductor substrate (self-supporting substrate (30)), wherein, it is made of III nitride semiconductor crystal, with a thickness of 300 μm or more and 1000 μm or less, the first main surface and the second main surface of exposing in positive back relationship are semi-polarity face, keep the m axis of X-ray and the III nitride semiconductor crystal incident in parallel respectively for first main surface and the second main surface and is measured XRC obtained (X-ray Rocking Curve, X-ray rocking curve) half breadth difference be 500arcsec or less.

Description

The manufacture of III nitride semiconductor substrate and III nitride semiconductor substrate Method
Technical field
The present invention relates to the manufacturing methods of a kind of III nitride semiconductor substrate and III nitride semiconductor substrate.
Background technique
Comprising using semi-polarity face as the substrate of the Group III nitride semiconductor layer of main surface, just in the development phase.In patent Relevant technology is disclosed in document 1.
Patent Document 1 discloses a kind of substrates, have the layer being made of III nitride semiconductor, this layer The normal of main surface is from [11-22] axial direction+c-axis direction with 5 degree or more and 17 degree range inclinations below.
As its manufacturing method, following method is disclosed: in the basal substrate (sapphire that main surface is defined face orientation Substrate, III nitride semiconductor substrate etc.) on, pass through MOCVD (metal organic chemical vapor Deposition, Metallo-Organic Chemical Vapor deposition) method, molecular beam epitaxy, HVPE (Hydride Vapor Phase Epitaxy, hydride gas-phase epitaxy) method etc., using the semi-polarity face with Ga polar component as aufwuchsplate, nitrogenize III group Layer as described above is consequently formed in object semiconductor epitaxial growth.
Prior art document
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2016-12717 bulletin.
Summary of the invention
The invention solves project
Technology as disclosed in Patent Document 1 is such, in the semi-polarity face that will have Ga polar component as aufwuchsplate In growth, as the thickness of growth increases (specifically 1mm or more), the X-ray of one of index as crystallinity evaluation The half breadth of rocking curve (XRC) is deteriorated.Therefore it is difficult to obtain the bulk crystals that crystallinity is excellent.
It is raw with the III nitride semiconductor of semi-polarity face main surface for making that the issue of the present invention is to provide a kind of Long new technology.
Means for solving the problems
A kind of III nitride semiconductor substrate is provided according to the present invention, wherein it is by III nitride semiconductor crystalline substance Body is constituted, with a thickness of 300 μm or more and 1000 μm hereinafter, the first main surface and the second main surface of the exposing in positive back relationship It is semi-polarity face, makes X-ray and the III nitride semiconductor respectively for first main surface and the second main surface The m axis of crystal is incident in parallel and is measured XRC's obtained (X-ray Rocking Curve, X-ray rocking curve) The difference of half breadth is 500arcsec or less.
In addition, providing a kind of manufacturing method of III nitride semiconductor substrate according to the present invention, wherein it includes base Plate preparatory process, the process prepare sapphire substrate；Heat treatment procedure, the process is after the substrate preparatory process, to institute Sapphire substrate is stated to be heat-treated；Pre- stream process, the process is after the heat treatment procedure, on Xiang Suoshu sapphire substrate Supply contains metal gas；Buffer layer formation process, the process is after the pre- stream process, on the sapphire substrate, In Under growth temperature is 800 DEG C or more and 950 DEG C or less, pressure is 30torr or more and 200torr growth conditions below, formed Buffer layer；First growth process, the process is after the buffer layer formation process, with Metalorganic Chemical Vapor Deposition, Growth temperature is 800 DEG C or more and 1025 DEG C or less, pressure is 30torr or more and 200torr or less, the speed of growth are 10 μ It under the growth conditions of m/h or more, grows III nitride semiconductor on the buffer layer, the first grown layer is consequently formed； With, second growth process, the process it is described first growth process after, group III-nitride is made with hydride vapour phase epitaxy method Semiconductor is grown on first grown layer, and the second grown layer is consequently formed.
The effect of invention
It is according to the present invention, it can be achieved that new for making to grow with the III nitride semiconductor of semi-polarity face main surface Technology.
Detailed description of the invention
By preferred embodiment as described below and its subsidiary the following drawings further elucidate above-mentioned purpose and other Objects, features and advantages.
Fig. 1 is one of the process flow for the manufacturing method of III nitride semiconductor substrate for indicating present embodiment The flow chart of example.
Fig. 2 is the side view for schematically showing an example of template substrate 20 for present embodiment.
Fig. 3 is the side view for schematically showing an example of self-supporting substrate 10 for present embodiment.
Fig. 4 is to schematically show to obtain by the manufacturing method of the III nitride semiconductor substrate of present embodiment Structural body an example side view.
Fig. 5 is to schematically show to obtain by the manufacturing method of the III nitride semiconductor substrate of present embodiment Structural body an example side view.
Fig. 6 is the side view for schematically showing an example of self-supporting substrate 30 for present embodiment.
Fig. 7 is the figure for indicating the characteristic of self-supporting substrate 10 and template substrate 20 of present embodiment.
Fig. 8 is the figure for indicating the characteristic of self-supporting substrate 30 of present embodiment.
Fig. 9 is the figure for indicating the characteristic of substrate of comparative example.
Figure 10 is the figure for indicating the characteristic of substrate of comparative example.
Specific embodiment
Hereinafter, using attached drawing to the III nitride semiconductor substrate and III nitride semiconductor of present embodiment The embodiment of the manufacturing method of substrate is illustrated.In addition, figure is merely used for illustrating the skeleton diagram of the composition of invention, respectively Size, shape, quantity, ratio of size of different components of component etc. are not limited to the content of diagram.
Firstly, the summary to present embodiment is illustrated.According to this embodiment party comprising characteristic a plurality of processes The manufacturing method of the III nitride semiconductor substrate of formula can be adopted with mocvd method, on sapphire substrate, with N polarity side Semi-polarity face (being indicated with Miller index (hkml), semi-polarity face of the l less than 0) lead group III-nitride partly as aufwuchsplate Body growth.As a result, the Group III nitride semiconductor layer that can get the semi-polarity face that exposed surface is N polarity side is located at sapphire Template substrate on substrate or propping up certainly from III nitride semiconductor obtained from template substrate removing sapphire substrate Support group plate.
Also, the manufacturing method of III nitride semiconductor substrate according to the present embodiment, can be in above-mentioned template substrate Or on self-supporting substrate, III nitride semiconductor thick film is made using the semi-polarity face of N polarity side as aufwuchsplate with HVPE method Growth.As a result, the bulk crystals of the III nitride semiconductor in the semi-polarity face that exposed surface is N polarity side can be obtained.
Details described below, but according to the manufacturing method, when growing III nitride semiconductor thick film, with The half breadth of the increase of growth thickness, the XRC of one of index as crystallinity evaluation hardly changes, or has and become good Tendency.Therefore, the excellent bulk crystals of crystallinity can be obtained.Then, it by being sliced etc. to bulk crystals, can obtain To the self-supporting substrate of most III nitride semiconductors.
Then, present embodiment is described in detail.Fig. 1 shows the systems of the III nitride semiconductor substrate of present embodiment Make an example of the process flow of method.As shown, there is substrate preparatory process S10, heat treatment procedure S20, flow work in advance Sequence S30, buffer layer formation process S40, the first growth process S50 and the second growth process S60.Although it is not shown, but second After growth process S60, it is possible to have cut out process.
In substrate preparatory process S10, prepare sapphire substrate.The diameter of sapphire substrate 10 is, for example, 1 inch or more. In addition, the thickness of sapphire substrate 10 is, for example, 250 μm or more.
The face orientation of the main surface of sapphire substrate is controlled at the Group III nitride semiconductor layer of epitaxial growth thereon One in a plurality of elements in the face orientation of aufwuchsplate.The face side of the aufwuchsplate of the element and Group III nitride semiconductor layer The relationship of position is shown below in an example.In substrate preparatory process S10, preparing main surface is desired face orientation Sapphire substrate.
The main surface of sapphire substrate is, for example, the face { 10-10 } or { 10-10 } is made to tilt predetermined angular towards prescribed direction Face.
Can be { 10-10 } for example towards the face of prescribed direction inclination predetermined angular makes { 10-10 } towards any direction With the inclined face of any angle being greater than in 0 ° and 0.5 ° or less range.
In addition, make { 10-10 } towards the face of prescribed direction inclination predetermined angular be also possible to make { 10-10 } towards with the face a Parallel direction is to be greater than 0 ° and less than the inclined face of any angle within the scope of 10.5 °.Alternatively, making { 10-10 } towards regulation The face of direction inclination predetermined angular is also possible to make { 10-10 } towards the direction parallel with the face a to be greater than 0 ° and 10.5 ° or less models Enclose the interior inclined face of any angle.For example, { 10-10 } is made to be also possible to make towards the face of prescribed direction inclination predetermined angular { 10-10 } towards the direction parallel with the face a with 0.5 ° or more and 1.5 ° or less, 1.5 ° or more and 2.5 ° or less, 4.5 ° or more and The inclined face of any angle in 5.5 ° or less, 6.5 ° or more and 7.5 ° or less, 9.5 ° or more and 10.5 ° or less ranges.
Heat treatment procedure S20 is carried out after substrate preparatory process S10.In heat treatment procedure S10, in condition below Under sapphire substrate is heat-treated.
Temperature: 800 DEG C or more and 1200 DEG C or less.
Pressure: 30torr or more and 760torr or less.
Heat treatment time: 5 minutes or more and 20 minutes or less.
Carrier gas: H2Or H2And N2(H2Ratio 0~100%).
Carrier gas supply amount: 3slm or more and 50slm or less (still, becomes due to supply amount according to the size of grower It is dynamic therefore without being limited thereto).
In addition, having the case where carrying out while carrying out nitrogen treatment to the heat treatment of sapphire substrate and without nitridation The case where handling and carrying out.In the case where being heat-treated while carrying out nitrogen treatment, in heat treatment, by 0.5slm Above and 20slm NH below3It is supplied on sapphire substrate and (still, is become due to supply amount according to the size of grower It is dynamic therefore without being limited thereto).In addition, not supplied in the case where being heat-treated without nitrogen treatment in heat treatment NH3。
The presence or absence of nitrogen treatment when heat treatment becomes control epitaxial growth in the main surface of sapphire substrate sometimes Group III nitride semiconductor layer aufwuchsplate face orientation a plurality of elements in one.The element and group III-nitride The relationship in the face orientation of the aufwuchsplate of semiconductor layer is shown below in an example.
Pre- stream process S30 is carried out after heat treatment procedure S20.In stream process S30 in advance, under the following conditions to blue precious Supply contains metal gas in the main surface of ground mass plate.For example, can carry out flowing process S30 in advance in MOCVD device.
Temperature: 500 DEG C or more and 1000 DEG C or less.
Pressure: 30torr or more and 200torr or less.
Trimethyl aluminium supply amount, service time: 20ccm or more and 500ccm are hereinafter, 60 seconds 1 second or more or less.
Carrier gas: H2Or H2And N2(H2Ratio 0~100%).
Carrier gas supply amount: 3slm or more and 50slm or less (wherein, size of the supply amount of gas according to grower, knot Structure and change, therefore be not limited to this).
Above-mentioned condition is the feelings as the trimethyl aluminium, triethyl aluminum that are supplied containing metal gas as organic metal raw material Condition.In this process, it can also supply and contain metal gas to replace trimethyl aluminium, triethyl aluminum, in indigo plant containing other metals Other metal films such as titanium film, vanadium film or copper film are formed in the main surface of jewel substrate to replace aluminium film.Alternatively, it is also possible to blue precious It is formed in the main surface of ground mass plate and is reacted as with the hydrocarbon compounds such as the methane, ethylene, the ethane that are generated by organic metal raw material Other metal-carbide films such as aluminium carbide, titanium carbide, vanadium carbide or the carbonization copper of film.
By flowing process S30 in advance, metal film, metal-carbide film are formed in the main surface of sapphire substrate.The metal film Presence be condition for inverting the polarity of the crystal grown on it.That is, implementing pre- stream process S30 is for making in indigo plant The face orientation of the aufwuchsplate of the Group III nitride semiconductor layer of epitaxial growth becomes N polarity side in the main surface of jewel substrate One in a plurality of elements in face.
Buffer layer formation process S40 is carried out after stream process S30 in advance.In buffer layer formation process S40, in sapphire Buffer layer is formed in the main surface of substrate.The thickness of buffer layer is, for example, 20nm or more and 300nm or less.
Buffer layer is, for example, AlN layers.For example, AlN crystal epitaxy can be made under the following conditions to form buffer layer.
Growing method: mocvd method.
Growth temperature: 800 DEG C or more and 950 DEG C or less.
Pressure: 30torr or more and 200torr or less.
Trimethyl aluminium supply amount: 20ccm or more and 500ccm or less.
NH3Supply amount: 0.5slm or more and 10slm or less.
Carrier gas: H2Or H2And N2(H2Ratio 0~100%).
Carrier gas supply amount: 3slm or more and 50slm or less (wherein, size of the supply amount of gas according to grower, knot Structure and change, therefore be not limited to this).
It is raw that the growth conditions of buffer layer formation process S40 becomes control extension in the main surface of sapphire substrate sometimes One in a plurality of elements in the face orientation of the aufwuchsplate of long Group III nitride semiconductor layer.The element and III group nitrogenize The relationship in the face orientation of the aufwuchsplate of object semiconductor layer is shown below in an example.
In addition, in buffer layer formation process S40 growth conditions (growth temperature as defined in lower, specifically 800 ~950 DEG C and lower pressure) it can be as the condition for growing AlN while maintaining N polarity.That is, buffer layer is formed Growth conditions in process S40 is the III nitride semiconductor for making the epitaxial growth in the main surface of sapphire substrate The face orientation of the aufwuchsplate of layer becomes one in a plurality of elements in the face of N polarity side.
First growth process S50 is carried out after buffer layer formation process S40.In the first growth process S50, following Make III nitride semiconductor crystal (for example, GaN crystal) epitaxial growth under growth conditions, on the buffer layer to form growth Face becomes the Group III nitride semiconductor layer (the first grown layer) in defined face orientation (the semi-polarity face of N polarity side).First is raw The thickness of long layer is, for example, 1 μm or more and 20 μm or less.
Growing method: mocvd method.
Growth temperature: 800 DEG C or more and 1025 DEG C or less.
Pressure: 30torr or more and 200torr or less.
TMGa supply amount: 25sccm or more and 1000sccm or less.
NH3Supply amount: 1slm or more and 20slm or less.
Carrier gas: H2Or H2And N2(H2Ratio 0~100%).
Carrier gas supply amount: 3slm or more and 50slm or less (wherein, size of the supply amount of gas according to grower, knot Structure and change, therefore be not limited to this).
Growth rate: 10 μm/h or more.
Growth conditions (relatively low growth temperature, relatively low pressure, relatively fast life in first growth process S50 Long rate) it can be as the condition for making GaN growth while maintaining N polarity.That is, the growth in the first growth process S50 Condition is the face side for making the aufwuchsplate of the Group III nitride semiconductor layer of epitaxial growth in the main surface of sapphire substrate Position is one of a plurality of elements in face of N polarity side.
As described above, stacking gradually sapphire substrate 21, buffer layer 22 and group III-nitride as shown in Fig. 2, can manufacture Semiconductor layer (the first grown layer 23), the face orientation of the aufwuchsplate 24 of the first grown layer 23 become the semi-polarity face of N polarity side Template substrate 20.In addition, the face orientation of aufwuchsplate 24 can be made to become by adjusting manufacturing condition in the range of above-mentioned condition Desired semi-polarity face.
In addition, as shown in Fig. 2, (first is raw obtaining sapphire substrate 21, buffer layer 22, Group III nitride semiconductor layer Long layer) 23 stack gradually made of after laminated body, by removing sapphire substrate 21 and buffer layer 22, can manufacture by such as Fig. 3 Shown in the first grown layer 23 constitute self-supporting substrate 10.
Means for removing sapphire substrate 21 and buffer layer 22 are not particularly limited.For example, can by using by Stress caused by linear expansion coefficient difference between sapphire substrate 21 and the first grown layer 23 separates them.Then, may be used To pass through the removal buffer layer 22 such as grinding, etching.
As another removal example, peeling layer can be formed between sapphire substrate 21 and buffer layer 22.For example, can also Carbide (aluminium carbide, titanium carbide, zirconium carbide, hafnium carbide, vanadium carbide or carbonization are dispersed with to be formed on sapphire substrate 21 Tantalum) carbon-coating and carbide (aluminium carbide, titanium carbide, zirconium carbide, hafnium carbide, vanadium carbide or tantalum carbide) layer laminated body after, Nitrogen treatment is carried out, using the layer formed after nitrogen treatment as peeling layer.
It is formed after buffer layer 22 and the first grown layer 23 on such peeling layer, when raw higher than being used to form first When heating the lamination under the conditions of the temperature of heating temperature when long layer 23, indigo plant can be separated into using the part of peeling layer as boundary The part of 23 side of part and the first grown layer of 21 side of jewel substrate.From the part of 23 side of the first grown layer, by grinding or losing Quarter etc. removes buffer layer 22 etc., it is hereby achieved that the self-supporting substrate 10 being made of the first grown layer 23 as shown in Figure 3.
Second growth process S60 is carried out after the first growth process S50.In the second growth process S60, above-mentioned The main table of first grown layer 23 of the first grown layer 23 or self-supporting substrate 10 (referring to Fig. 3) of template substrate 20 (referring to Fig. 2) On face (the semi-polarity face of N polarity side), III nitride semiconductor crystal (such as: GaN crystal) is made with growth conditions below Epitaxial growth, forming aufwuchsplate becomes the Group III nitride semiconductor layer in defined face orientation (the semi-polarity face of N polarity side) (the second grown layer).The thickness of second grown layer is, for example, 1.0mm or more.
Growing method: HVPE method.
Growth temperature: 900 DEG C or more and 1100 DEG C or less.
Growth time: 1 hour or more.
V/III ratio: 1 or more and 20 or less.
Grow film thickness: 1.0mm or more.
In addition, the second growth process S60 can also be carried out discontinuously, and it is divided into a plurality of steps and carries out.For example, It is temporarily cooling after regulation film thickness being grown into HVPE method, regulation film thickness is then grown into HVPE method again.In first step It is temporarily cooling after middle formation Group III nitride semiconductor layer, it will be cracked in the Group III nitride semiconductor layer.By This, internal stress is alleviated.Then, when making III nitride semiconductor in the Group III nitride semiconductor layer with crackle When epitaxial growth, crackle is clipped and separated crystal mutually merges with growth each other.Moreover, because slow by above-mentioned cooling With internal stress, therefore even if thick-film, bulk crystals are also not susceptible to crackle.
In addition, the second growth process S60 can also make template substrate 20 or self-supporting substrate 10 be fixed on carbon pedestal etc. It is directly carried out in the state of pedestal.Thereby, it is possible to inhibit as second growth process S60 in heating caused by template substrate 20 or The deformation of self-supporting substrate 10.In addition, instantiating the method for the bonding agent using alumina series as the method for fixing it Deng, but not limited to this.By these characterization methods, it is 50mm or more and 4 inch of major diameter below that maximum gauge, which may be implemented, Bulk crystals.
By the above, the laminated body (referring to Fig. 4) with template substrate 20 and the second grown layer 25 can be obtained or had The laminated body of self-supporting substrate 10 and the second grown layer 25 (referring to Fig. 5).
What is carried out after the second growth process S60 cuts out in process, by from including that the first grown layer 23 and second are raw The bulk crystals of long layer 25 cut Group III nitride semiconductor layer with slice etc., obtain by Group III nitride semiconductor layer structure At self-supporting substrate 30 (referring to Fig. 6).The Group III nitride semiconductor layer cut by slice etc. both can be only by the second growth Layer 25 is constituted, and be may also comprise the first grown layer 23 and the second grown layer 25, can be also only made of the first grown layer 23.
But the first grown layer 23 and second is preferably comprised by the Group III nitride semiconductor layer that slice etc. is cut In the bulk crystals of grown layer 25 growth thickness (using the growth start time of the first grown layer 23 as 0 calculate thickness) be The part of 3mm or more.The reason for this is that brilliant intracorporal dislocation defect is about 1 × 107cm-2Or less than 1 × 107cm-2, as Device substrate and have quality appropriate.
Then, the composition and feature of the self-supporting substrate 30 obtained by the above-mentioned manufacture method are illustrated.
According to this embodiment party for growing III nitride semiconductor thick film as aufwuchsplate using the semi-polarity face of N polarity side The manufacturing method of formula, as the thickness of growth increases, the half breadth of the XRC of one of index as crystallinity evaluation is shown The tendency for hardly changing or improving at leisure.The self-supporting substrate 30 of present embodiment shows the feature due to the tendency. In addition, the tendency is (to be indicated different from the semi-polarity face with Ga polarity side with Miller index (hkml), l is greater than 0 semi-polarity Face) make as aufwuchsplate III nitride semiconductor thick film grow the case where a kind of tendency.
Firstly, the self-supporting substrate 30 of present embodiment is made of III nitride semiconductor crystal, in positive back relationship Exposing the first main surface and the second main surface be semi-polarity face.
Moreover, as shown in embodiment below, out of, bulk crystals comprising the first grown layer 23 and the second grown layer 25 Growth thickness be 3mm or more the obtained self-supporting substrate 30 in part, even if with a thickness of 300 μm or more and 1000 μm hereinafter, Also it can make the m axis of X-ray and III nitride semiconductor crystal respectively for the first main surface and the second main surface in parallel Difference that is incident and being measured the half breadth of XRC obtained is 500arcsec or less.
In addition, the first main surface and the second main surface all show it is wide to the half value for the XRC that m axis is incident in parallel and measures Degree is 500arcsec good numerical value below.
In addition, as shown in embodiment below, out of, bulk crystals comprising the first grown layer 23 and the second grown layer 25 Growth thickness be 3mm or more the obtained self-supporting substrate 30 in part, even if with a thickness of 300 μm or more and 1000 μm hereinafter, Also it can make the projection of the c-axis of X-ray and III nitride semiconductor crystal respectively for the first main surface and the second main surface Axis is incident in parallel and is measured the difference of the half breadth of XRC obtained as 500arcsec or less.
In addition, the first main surface and the second main surface all show incident in parallel with the axis of projection of c-axis and are measured The half breadth of XRC obtained is 500arcsec good numerical value below.
In this way, the self-supporting substrate 30 of present embodiment is " incident in parallel with the axis of projection of c-axis and be measured and obtained XRC half breadth " and the two of " incident in parallel with m axis and be measured the half breadth of XRC obtained " in Show good numerical value.
In addition, nitrogenizing III group as aufwuchsplate using the semi-polarity face of Ga polarity side as shown in embodiment below In the case that object semiconductor thick film is grown, as the thickness of growth increases, the half of the XRC of one of index as crystallinity evaluation Value width can be deteriorated.Part especially more than growth thickness 1mm, which starts to show significantly, in growth thickness 3mm Above part, crystallinity are significantly deteriorated, and the half breadth that calculate above-mentioned XRC becomes difficult.As one of its reason, it is believed that When being grown using the semi-polarity face of Ga polarity side as aufwuchsplate, the introduction volume of oxygen atom unexpectedly increases, the crystalline substance of crystal Lattice constant changes, and dislocation defects increase.
In addition, as described above, the maximum gauge of the bulk crystals manufactured with features described above manufacturing method greatly to 50mm with It is upper and 4 inches or less.The self-supporting substrate of the present embodiment as obtained from being cut out from such bigbore bulk crystals 30 become maximum gauge also as 50mm or more and 4 inch of heavy caliber below.
[embodiment]
< first evaluates >
In the first evaluation, be identified through meet it is above-mentioned whole " for making the growth of Group III nitride semiconductor layer The face orientation in face becomes a plurality of elements in the face of N polarity side ", the face of the aufwuchsplate of Group III nitride semiconductor layer can be made Orientation becomes the face of N polarity side.In addition, be unsatisfactory for it is above-mentioned " for making the face of the aufwuchsplate of Group III nitride semiconductor layer In the case where at least one of a plurality of elements of orientation as the face of N polarity side ", Group III nitride semiconductor layer is confirmed Aufwuchsplate face orientation be Ga polarity side face.
Firstly, the face orientation for preparing main surface is to have tilted 2 ° from the face m (face (10-10)) to the direction parallel with the face a The sapphire substrate in face.Sapphire substrate with a thickness of 430 μm, diameter is 2 inches.
Then, under the following conditions, heat treatment procedure S20 is implemented to ready sapphire substrate.
Temperature: 1000~1050 DEG C.
Pressure: 100torr.
Carrier gas: H2、N2。
Heat treatment time: 10 minutes or 15 minutes.
Carrier gas supply amount: 15slm.
It should be noted that supplying the NH of 20slm in heat treatment procedure S203, carry out nitrogen treatment.
Then, under the following conditions, pre- stream process S30 has been carried out.
Temperature: 800~930 DEG C.
Pressure: 100torr.
Trimethyl aluminium supply amount, service time: 90sccm, 10 seconds.
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
Then, buffer layer formation process S40 is carried out under the following conditions, forms AlN layers.
Growing method: mocvd method.
Growth temperature: 800~930 DEG C.
Pressure: 100torr.
Trimethyl aluminium supply amount: 90sccm.
NH3Supply amount: 5slm.
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
Then, the first growth process S50 is carried out under the following conditions, forms Group III nitride semiconductor layer.
Growing method: mocvd method.
Pressure: 100torr.
TMGa supply amount: 50~500sccm (consecutive variations).
NH3Supply amount: 5~10slm (consecutive variations).
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
Growth rate: 10 μm/h or more.
In addition, the growth temperature control of the first sample is at 900 DEG C ± 25 DEG C, the growth temperature of the second sample is controlled 1050 ℃±25℃.That is, the first sample is to meet above-mentioned whole " for making the face side of the aufwuchsplate of Group III nitride semiconductor layer The sample of a plurality of elements of the position as the face of N polarity side ".Second sample be unsatisfactory for it is above-mentioned " for making group III-nitride half A part (the first growth process S50 in a plurality of elements of the face orientation of the aufwuchsplate of conductor layer as the face of N polarity side " In growth temperature) sample.
The face orientation of the aufwuchsplate of the Group III nitride semiconductor layer of first sample is from (- 1-12-4) towards the face side-a 8.5 ° of faces below are tilted to 5.0 ° of inclination and to the direction parallel with the face m.On the other hand, the group III-nitride of the second sample The face orientation of the aufwuchsplate of semiconductor layer is to tilt 5.0 ° towards the face a direction from (11-24) and tilt to the direction parallel with the face m 8.5 ° of faces below.I.e., it is known that by whether meeting above-mentioned " for making the face of the aufwuchsplate of Group III nitride semiconductor layer Orientation becomes a plurality of elements in the face of N polarity side ", the face orientation that can adjust aufwuchsplate, which becomes Ga polarity, still becomes the pole N Property.
The XRD pole measurement result in face (- 1-12-4) or the face (11-24) in the first sample is shown in Fig. 7.It can be confirmed Diffraction maximum is that the position in several years is offset by from the central point of pole.If the deviation of measurement angle in detail, can be confirmed it is-a 5.0 ° of the position or the face a direction in 5.0 ° of face direction and the direction 8.5 ° parallel with the face m and the direction 8.5 ° parallel with the face m Position.
In addition, the inventors of the present invention confirmed, be unsatisfactory for it is above-mentioned " for making the aufwuchsplate of Group III nitride semiconductor layer Face orientation become N polarity side face a plurality of elements " in other a part in the case where, or all ungratified feelings Under condition, the face orientation of aufwuchsplate can also become Ga polarity.
< second evaluates >
In the second evaluation, it is above-mentioned " for adjusting the aufwuchsplate of Group III nitride semiconductor layer to be identified through adjustment A plurality of elements in face orientation " can adjust the face orientation of the aufwuchsplate of Group III nitride semiconductor layer.
Firstly, the face orientation for preparing a plurality of main surfaces is various sapphire substrates.The thickness of sapphire substrate It is 430 μm, diameter is 2 inches.
Then, under the following conditions, heat treatment procedure S20 has been carried out respectively to ready each sapphire substrate.
Temperature: 1000~1050 DEG C.
Pressure: 200torr.
Heat treatment time: 10 minutes.
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
In addition, different sample in terms of having made in heat treatment whether there is or not nitrogen treatment.Specifically, having made in Re Chu The NH of 20slm is supplied when reason3And it carries out the sample of nitrogen treatment and does not supply NH in heat treatment3And without nitrogen treatment Both samples of sample.
Then, pre- stream process S30 is carried out under the following conditions.
Temperature: 880~930 DEG C.
Pressure: 100torr.
Trimethyl aluminium supply amount, service time: 90sccm, 10 seconds.
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
In addition, having made the sample for carrying out pre- stream process S30 and both samples without flowing process S30 in advance.
Then, forming thickness in the main surface of sapphire substrate (exposed surface) under the following conditions is about the slow of 150nm Rush layer (AlN buffer layer).
Growing method: mocvd method.
Pressure: 100torr.
V/III ratio: 5184.
TMAl supply amount: 90ccm.
NH3Supply amount: 5slm.
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
In addition, keeping the growth temperature of each sample different but in 700 DEG C or more and 1110 DEG C or less of range.
Then, the Group III nitride semiconductor layer that thickness is about 15 μm is formd on the buffer layer under the following conditions (GaN layer).
Growing method: mocvd method.
Growth temperature: 900~1100 DEG C.
Pressure: 100torr.
V/III ratio: 321.
TMGa supply amount: 50~500ccm (oblique ascension).
NH3Supply amount: 5~10slm (oblique ascension).
Carrier gas: H2、N2。
Carrier gas supply amount: 15slm.
As described above, having manufactured made of stacking gradually sapphire substrate, buffer layer and Group III nitride semiconductor layer III nitride semiconductor substrate 1.
Show that " a plurality of of face orientation for adjusting the aufwuchsplate of Group III nitride semiconductor layer want in table 1~7 The relationship of element " and the face orientation of the aufwuchsplate of Group III nitride semiconductor layer.
[table 1]
[table 2]
[table 3]
[table 4]
[table 5]
[table 6]
[table 7]
In " sapphire main surface " column in table, the face orientation of the main surface of sapphire substrate is shown.In " heating When nitrogen treatment " in a column, whether there is or not the nitrogen treatment (" having " or "None") when heating when showing heat treatment procedure S20.In In " whether there is or not trimethyl aluminiums to flow process in advance " column, show that whether there is or not trimethyl aluminiums to flow process (" having " or "None") in advance." AlN is slow Rush growth temperature " in a column, show the growth temperature in buffer layer formation process.In " GaN growth temperature " column, show Growth temperature in GaN layer formation process.In " aufwuchsplate of Group III nitride semiconductor layer " column, III group is shown The face orientation of the aufwuchsplate of nitride semiconductor layer.
According to the result it is found that by adjusting above-mentioned " for adjusting the face of the aufwuchsplate of Group III nitride semiconductor layer A plurality of elements in orientation " can adjust the face of the aufwuchsplate of Group III nitride semiconductor layer among semi-polarity and Ga polarity Orientation.Also, according to the result of the first evaluation and the result of the second evaluation it is found that in satisfaction whole " for nitrogenizing III group The face orientation of the aufwuchsplate of object semiconductor layer becomes a plurality of elements in the face of N polarity side " on the basis of, by adjusting " being used for Adjust a plurality of elements in the face orientation of the aufwuchsplate of Group III nitride semiconductor layer ", it can be among semi-polarity and N polarity Adjust the face orientation of the aufwuchsplate of Group III nitride semiconductor layer.
< third evaluates >
In third evaluation, with the crystallinity of the half breadth evaluation self-supporting substrate 30 of XRC.
Embodiment 1
Firstly, with mocvd method, on there is the m surface sapphire substrate to the deflecting angle in 2 ° of the face a direction, via buffer layer, It is formed GaN layer (the first grown layer 23).The main surface (exposed surface) of first grown layer 23 is the semi-polarity face ({ -1- of N polarity side 12-4 } face (+α ° of deflecting angle)).In addition, the thickness of the first grown layer 23 is about 15 μm.
Then, on the first grown layer 23, with HVPE method growing gan crystal, the GaN layer (second of thickness about 11mm is formed Grown layer 25).Then, by being by the growth thickness in the bulk crystals being made of the first grown layer 23 and the second grown layer 25 The part of 3mm or more is vertically sliced in the direction of growth, obtains plural number semi-polarity substrate.
Then, GaN (11-22) face diffraction XRC measurement is implemented to each sample.It is incident in parallel with X-ray and m axis Mode and incident mode, both modes are determined in parallel with the axis of projection of c-axis.
Fig. 8 shows the results of GaN (11-22) face diffraction XRC measurement.The horizontal axis of figure indicates that (slice obtains growth film thickness The position that the slave bulk crystals of semi-polarity substrate are cut out).The longitudinal axis of figure indicates GaN (11-22) XRC half breadth.
In embodiment 1, it is known that X-ray and m axis it is incident in parallel and be measured the half breadth of XRC obtained and The axis of projection of X-ray and c-axis is incident in parallel and is measured the half breadth of XRC obtained, with the increasing of growth film thickness Add and all hardly changes or with the tendency to improve at leisure.
It is incident in parallel with m axis and be measured and obtained moreover, in the range of growing 3000 μm~10000 μm of film thickness The half breadth of the XRC obtained is in 500arcsec hereinafter, it is preferred that in 300arcsec hereinafter, more preferably in 250arcsec or less.Together Sample, in the range, half breadth that is incident and being measured XRC obtained is in parallel with the axis of projection of c-axis 500arcsec hereinafter, preferably 300arcsec hereinafter, more preferably 200arcsec hereinafter, further preferably 150arcsec Below.
In addition, as seen from the figure, for the part that the growth thickness in bulk crystals is 3mm or more is hung down in the direction of growth 300 μm of thickness or more and 1000 μm of semi-polarity substrates below obtained from directly being sliced, respectively for the first main surface and Two main surfaces (front and back) keep the m axis of X-ray and III nitride semiconductor crystal incident in parallel and are measured institute The difference of the half breadth of the XRC of acquisition is 500arcsec hereinafter, preferably 300arcsec is hereinafter, more preferably 250arcsec Hereinafter, further preferably 150arcsec or less.
In addition, as seen from the figure, for the part that the growth thickness in bulk crystals is 3mm or more is hung down in the direction of growth 300 μm of thickness or more and 1000 μm of semi-polarity substrates below obtained from directly being sliced, respectively for the first main surface and Two main surfaces (front and back) keep the axis of projection of the c-axis of X-ray and III nitride semiconductor crystal incident in parallel and into It is 500arcsec hereinafter, preferably 300arcsec is hereinafter, more preferably that row, which measures the difference of the half breadth of XRC obtained, 200arcsec hereinafter, further preferably 150arcsec hereinafter, further preferably 100arcsec or less.
In addition, also know, if make with a thickness of 300 μm or more and 500 μm hereinafter, if respectively for the first main surface and second Main surface (front and back) keeps the m axis of X-ray and III nitride semiconductor crystal incident in parallel and is measured and is obtained XRC half breadth difference and half value that is incident and being measured XRC obtained is wide in parallel with the axis of projection of c-axis The difference of degree is 200arcsec or less.
Comparative example 1
GaN layer is formed via buffer layer on the positive face m (just m-plane) sapphire substrate with mocvd method.GaN layer Main surface (exposed surface) is the semi-polarity face (face (11-22)) of Ga polarity side.The thickness of GaN layer is about 1 μm.
Then, in above-mentioned GaN layer, about 15 μm of thickness of GaN layer is formed with HVPE method.At this point, X-ray and III group nitrogen The half breadth for GaN (11-22) XRC that the m axis of compound semiconductor crystal is incident in parallel and measures is 955arcsec.In addition, The half of GaN (11-22) XRC that the axis of projection of the c-axis of X-ray and III nitride semiconductor crystal is incident in parallel and measures Value width is 461arcsec.
In turn, the GaN layer of thickness about 1.5mm is formed in above-mentioned GaN layer.Then, it is obtained to mocvd method and HVPE method The bulk crystals being made of GaN layer be ground, attrition process, obtain semi-polarity substrate.
Here, Fig. 9 indicates the m axis of X-ray and III nitride semiconductor crystal in the semi-polarity substrate of comparative example 1 Incident and GaN (11-22) XRC of measurement measurement result in parallel.Figure 10 indicates that the X in the semi-polarity substrate of comparative example 1 is penetrated The measurement knot for GaN (11-22) XRC that the axis of projection of the c-axis of line and III nitride semiconductor crystal is incident in parallel and measures Fruit.As shown in these figures, crystallographic axis becomes a plurality of peaks towards various directions.I.e., it is known that in the face (11-22), the crystal of GaN layer is raw In length, if the film thickness of GaN layer becomes larger, there are the tendencies that the orientation of crystal is disintegrated.In addition, for being cut out by such crystal Substrate, the difference of the XRC half breadth between the first main surface and the second main surface can not be defined, or know its difference be greater than embodiment 1。
< the 4th evaluates >
Then, it is identified through the manufacturing method of present embodiment, can be obtained using semi-polarity face as main surface, maximum gauge For 4 inches of 50mm or more bigbore self-supporting substrates 30 below.
Firstly, having prepared on the sapphire substrate 21 that diameter is 4 inches of Φ, the face orientation of main surface is the face m via slow Rush the template 20 that layer 22 is formed with GaN layer (the first grown layer 23) with mocvd method.The face orientation of the main surface of first grown layer 23 For (- 1-12-3), maximum gauge is 4 inches of Φ.
Then, which is fixed on carbon pedestal.Specifically, using alumina series adhesive by process for sapphire-based The back side of plate 21 fits to the main surface of carbon pedestal.
Then, in the state of making template substrate 20 be fixed on carbon pedestal, in the main surface of the first grown layer 23 with HVPE method grows III nitride semiconductor (GaN).The GaN being made of the III nitride semiconductor of monocrystalline is formed as a result, Layer (a part of the second grown layer 25).Growth conditions is as follows.
Growth temperature: 1040 DEG C.
Growth time: 15 hours.
V/III ratio: 10.
Grow film thickness: 4.4mm.
Then, the stacking of a part comprising carbon pedestal, template substrate 20 and the second grown layer 25 is taken out from HVPE device Body is cooled to room temperature.Laminated body after cooling is observed, there are crackles on surface.In addition, being attached with along the periphery of above-mentioned laminated body Polycrystalline III nitride semiconductor, they are connected with each other and become ring-type, and above-mentioned laminated body is held within portion.
Then, in the state of the III nitride semiconductor of remaining polycrystalline, there are the GaN layer of crackle (second growth Layer 25 a part) main surface on HVPE method make III nitride semiconductor (GaN) grow.It is formed as a result, by monocrystalline The GaN layer (another part of the second grown layer 25) that III nitride semiconductor is constituted.Growth conditions is as follows.
Growth temperature: 1040 DEG C.
Growth time: 14 hours.
V/III ratio: 10.
Grow film thickness: 3.0mm (total film thickness of the second grown layer 25 is 7.4mm).
The maximum gauge of second grown layer 25 is about 4 inches of Φ.In addition, comprising the second grown layer 25 and along its periphery The maximum gauge in the face of polycrystalline III nitride semiconductor is about 130mm.It is split in addition, not generated in the second grown layer 25 Line.
Then, the second grown layer 25 is sliced, obtains a plurality of self-supporting substrates 30.It is not produced on self-supporting substrate 30 Raw crackle, maximum gauge is about 4 inches of Φ.
Hereinafter, the example of note reference mode.
1. a kind of III nitride semiconductor substrate, wherein
It is made of III nitride semiconductor crystal, with a thickness of 300 μm or more and 1000 μm hereinafter, closing in positive back The first main surface and the second main surface of the exposing of system are semi-polarity face,
Make X-ray and the III nitride semiconductor crystal respectively for first main surface and the second main surface M axis it is incident in parallel and to be measured the difference of the half breadth of X-ray rocking curve obtained be 500arcsec or less.
2. the III nitride semiconductor substrate according to 1, wherein
Make X-ray and the III nitride semiconductor crystal respectively for first main surface and the second main surface M axis it is incident in parallel and to be measured the difference of the half breadth of X-ray rocking curve obtained be 300arcsec or less.
3. according to III nitride semiconductor substrate described in 1 or 2, wherein
Keep X-ray parallel with the m axis of III nitride semiconductor crystal first main surface and the second main surface Ground is incident and to be measured the half breadth of X-ray rocking curve obtained be 500arcsec or less.
4. the III nitride semiconductor substrate according to any one of 1 to 3, wherein
Make X-ray and the III nitride semiconductor crystal respectively for first main surface and the second main surface C-axis axis of projection it is incident in parallel and the difference that is measured the half breadth of X-ray rocking curve obtained is 500arcsec or less.
5. the III nitride semiconductor substrate according to 4, wherein
Make X-ray and the III nitride semiconductor crystal respectively for first main surface and the second main surface C-axis axis of projection it is incident in parallel and the difference that is measured the half breadth of X-ray rocking curve obtained is 300arcsec or less.
6. according to III nitride semiconductor substrate described in 4 or 5, wherein
Make the throwing of the c-axis of X-ray and III nitride semiconductor crystal for first main surface and the second main surface The axis of shadow is incident in parallel and to be measured the half breadth of X-ray rocking curve obtained be 500arcsec or less.
7. a kind of manufacturing method of III nitride semiconductor substrate, wherein
It is included
Substrate preparatory process, the process prepare sapphire substrate；
Heat treatment procedure, the process are heat-treated the sapphire substrate after the substrate preparatory process；
Pre- stream process, the process is after the heat treatment procedure, and supply contains metal gas on Xiang Suoshu sapphire substrate；
Buffer layer formation process, the process is after the pre- stream process, on the sapphire substrate, in growth temperature For 800 DEG C or more and 950 DEG C or less, under pressure is 30torr or more and 200torr growth conditions below, form buffer layer；
First growth process, the process is after the buffer layer formation process, with Metalorganic Chemical Vapor Deposition, Growth temperature is 800 DEG C or more and 1025 DEG C or less, pressure is 30torr or more and 200torr or less, the speed of growth are 10 μ It under the growth conditions of m/h or more, grows III nitride semiconductor on the buffer layer, the first grown layer is consequently formed； With,
Second growth process, the process make III group nitrogen after the first growth process with hydride vapour phase epitaxy method Compound semiconductor is grown on first grown layer, and the second grown layer is consequently formed.
8. the manufacturing method of III nitride semiconductor substrate according to 7, wherein
It, which also has, cuts out process, and the process is from the bulk crystals comprising first grown layer and second grown layer Cut out III nitride semiconductor substrate.
9. the manufacturing method of III nitride semiconductor substrate according to 8, wherein
It is cut out in process described, cuts out the III from the part that the growth thickness in the bulk crystals is 3mm or more Group-III nitride semiconductor substrate.
This application claims excellent based on Japanese publication Patent 2017-064486 submitted based on March 29th, 2017 It first weighs, the disclosure of which is fully incorporated herein.

Claims (9)

1. a kind of III nitride semiconductor substrate, wherein
It is made of III nitride semiconductor crystal, with a thickness of 300 μm or more and 1000 μm hereinafter, in positive back relationship The first main surface and the second main surface exposed are semi-polarity face,
Make the m axis of X-ray Yu the III nitride semiconductor crystal respectively for first main surface and the second main surface Difference that is incident in parallel and being measured the half breadth of X-ray rocking curve obtained is 500arcsec or less.
2. III nitride semiconductor substrate according to claim 1, wherein
Make the m axis of X-ray Yu the III nitride semiconductor crystal respectively for first main surface and the second main surface Difference that is incident in parallel and being measured the half breadth of X-ray rocking curve obtained is 300arcsec or less.
3. III nitride semiconductor substrate according to claim 1 or 2, wherein
Enter X-ray and the m axis of III nitride semiconductor crystal in parallel first main surface and the second main surface The half breadth for penetrating and being measured X-ray rocking curve obtained is 500arcsec or less.
4. III nitride semiconductor substrate according to any one of claim 1 to 3, wherein
Make the c-axis of X-ray Yu the III nitride semiconductor crystal respectively for first main surface and the second main surface Axis of projection it is incident in parallel and be measured the difference of the half breadth of X-ray rocking curve obtained be 500arcsec with Under.
5. III nitride semiconductor substrate according to claim 4, wherein
Make the c-axis of X-ray Yu the III nitride semiconductor crystal respectively for first main surface and the second main surface Axis of projection it is incident in parallel and be measured the difference of the half breadth of X-ray rocking curve obtained be 300arcsec with Under.
6. III nitride semiconductor substrate according to claim 4 or 5, wherein
Make the axis of projection of the c-axis of X-ray and III nitride semiconductor crystal for first main surface and the second main surface It is incident in parallel and to be measured the half breadth of X-ray rocking curve obtained be 500arcsec or less.
7. a kind of manufacturing method of III nitride semiconductor substrate, wherein
It is included
Substrate preparatory process, the process prepare sapphire substrate；
Heat treatment procedure, the process are heat-treated the sapphire substrate after the substrate preparatory process；
Pre- stream process, the process is after the heat treatment procedure, and supply contains metal gas on Xiang Suoshu sapphire substrate；
Buffer layer formation process, the process on the sapphire substrate, are in growth temperature after the pre- stream process 800 DEG C or more and 950 DEG C or less, pressure be to form buffer layer under 30torr or more and 200torr growth conditions below；
First growth process, the process is after the buffer layer formation process, with Metalorganic Chemical Vapor Deposition, in life Long temperature is 800 DEG C or more and 1025 DEG C or less, pressure is 30torr or more and 200torr or less, the speed of growth are 10 μm/h It under above growth conditions, grows III nitride semiconductor on the buffer layer, the first grown layer is consequently formed；With,
Second growth process, the process make group III-nitride after the first growth process with hydride vapour phase epitaxy method Semiconductor is grown on first grown layer, and the second grown layer is consequently formed.
8. the manufacturing method of III nitride semiconductor substrate according to claim 7, wherein
It, which also has, cuts out process, which cuts out from the bulk crystals comprising first grown layer and second grown layer III nitride semiconductor substrate.
9. the manufacturing method of III nitride semiconductor substrate according to claim 8, wherein
It is cut out in process described, cuts out the III group nitrogen from the part that the growth thickness in the bulk crystals is 3mm or more Compound semiconductor substrate.
CN201880021145.6A 2017-03-29 2018-03-19 The manufacturing method of III nitride semiconductor substrate and III nitride semiconductor substrate Pending CN110462113A (en)

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